CN106700440B - A kind of heat conductive flame-retarding polyester composite and preparation method thereof - Google Patents
A kind of heat conductive flame-retarding polyester composite and preparation method thereof Download PDFInfo
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- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08K5/04—Oxygen-containing compounds
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- C08K5/00—Use of organic ingredients
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
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- C08K5/524—Esters of phosphorous acids, e.g. of H3PO3
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Abstract
The present invention provides a kind of heat conductive flame-retarding polyester composite and preparation method thereof, which is characterized in that its composition by weight is as follows: polyester resin 100；It is heat-treated magnesium hydroxide 100~300；Auxiliary heat conduction agent 0~50；Auxiliary flame retardant 0~30；Dispersing agent 1~8；Stabilizer 1~3.The present invention uses the heat treatment magnesium hydroxide for having superior heating conduction than common magnesium hydroxide and not losing flame retardant property, and auxiliary heat conduction agent and fire retardant, the more excellent heat conductive flame-retarding polyester composite of processability can meet various application requirements.
Description
Technical field:
A kind of heat conductive flame-retarding polyester composite and preparation method thereof is related to a kind of side for improving magnesium hydroxide heating conduction
Method can make polyester material by magnesium hydroxide prepared by this kind of method while have thermally conductive and flame retardant property.
Background technique:
Common polyester plastics mainly has polyethylene terephthalate (PET) and polybutylene terephthalate (PBT),
Since it is with excellent mechanical property, thermal stability, electrical insulating property, it is widely used in packing business, electronic apparatus, medical treatment are defended
The fields such as life, building, automobile.However, there is inflammable and poor thermal conductivity in polyester plastics itself, it is difficult to meet high-performance system
The application requirement of product, limit its Contemporary Industrial Design and manufacture in application range, therefore, research and development have it is fire-retardant and
The polyester composite of the performances such as thermally conductive is of great significance.
Flame retardant polyester is to be blended to be plasticized compound preparation by polyester base plastic and fire retardant, and main fire retardant has
The halogen flame retardant system of bromine based compound and antimony oxide composition, phosphorus series compound, metal hydroxides.Halogen flame is to polyester
It is hindered with good flame retardant effect, such as Chinese patent 201010612307.9 using decabromodiphenylethane, brominated triazine, phosphorus nitrogen
Two or more in combustion agent, tetrabromobisphenol A are compound for antimony oxide and/or sodium antimonate with fire retarding synergist, prepare resistance to burn
The PBT that heated filament is had excellent performance, flame retardant property is up to UL94 V-0, since in combustion process, bromine antimony based flame retardant can be generated to ring
Border harmful substance is just limited by more and more policies and regulations.
Phosphorus flame retardant meets environmental requirement, based on phosphate compounds, has the advantages that flame retarding efficiency is high, such as
Chinese patent 201210158866.6 uses tricresyl phosphate, antimony oxide as fire retardant, based on PBT, POM be
It is auxiliary, and using calcium carbonate, silica as filler, be prepared for a kind of enhancing anti-flaming PBT composite, have fire-retardant, high temperature resistant,
Antistatic, the features such as toughness is high.However phosphate is there are migration problem, this cause the anti-flammability of fire-retardant product and mechanical property with
Time reduces.
Thermally conductive polyester composite is to be blended to be plasticized compound acquisition by polyester base plastic and conduction powder, insulating properties without
Machine conduction powder mainly includes metal oxide (aluminium oxide, magnesia), nitride (such as boron nitride, aluminium nitride).Such as China
Patent 201510718473.X is prepared for a kind of thermally conductive using the mixture of magnesia, aluminium oxide and boron nitride as heat filling
PET alloy material.Metal oxide aluminium, oxidation magnesium hardness are high, and when extrusion is big to equipment attrition, and when high filling squeezes out is easy
The problems such as discoloration, limits it and uses as main conductive filler powder；Although nitride excellent thermal conductivity, in the polymer
It is difficult to disperse, additive amount is difficult to reach the requirement of thermally conductive threshold value, and expensive.
Chinese patent CN201610098700.8 by with the heat fillings such as graphene oxide, carbon nanotube and aluminium nitride,
Using compounding as fire retardant for borate and metal hydroxides, it is prepared for a kind of thermally conductive toughening flame-proof enhancing PBT plastic.However specially
The heat filling aluminium nitride and resin compatible selected in benefit are poor, and poor processability is difficult to realize high thermal conductivity under low filling；Carbon is received
It although mitron excellent thermal conductivity, can only apply and black products, be limited its scope of application from color；Magnesium hydroxide
As a kind of common halogen-free flame retardants, have the advantages that environmentally friendly, cheap, but its flame retarding efficiency is poor, while heat transfer efficiency
It is low.
Using limitation existing for heat conductive flame-retarding polyester composite wood for the preparation of the above all kinds of patents, this patent provides one kind
The method for promoting magnesium hydroxide heating conduction, the magnesium hydroxide heating conduction as made from this method is more than common magnesium hydroxide
Height, while flame retardant property is had both, the heat conductive flame-retarding polyester composite of preparation is had excellent performance, and can meet various application requirements.
Summary of the invention:
The present invention improves its heating conduction, provides a kind of tool for polyester resin matrix by heat treatment magnesium hydrate powder
The inorganic heat filling of standby anti-flammability and heating conduction, to prepare a kind of heat conductive flame-retarding polyester composite.
The present invention provides a kind of preparation method of heat conductive flame-retarding polyester composite, it is characterised in that it includes following components
(in terms of mass fraction):
Polyester resin 100
It is heat-treated magnesium hydroxide 100~300
Auxiliary heat conduction agent 0~50
Auxiliary flame retardant 0~30
Dispersing agent 1~8
Stabilizer 1~3
Above-mentioned various raw materials are added in high speed agitator and are mixed 5~30 minutes, mixture obtained is sent into twin-screw
Extruder melt pelletization, the temperature in each area of extruder are as follows: T1=190~200 DEG C, T2=195~205 DEG C, T3=200~210
DEG C, T4=205~215 DEG C, T5=210~220 DEG C, T6=215~225 DEG C, T7=220~230 DEG C, T8=225~235
DEG C, T9=230~240 DEG C, mould=220~230 DEG C T.
A kind of preparation method of heat conductive flame-retarding polyester composite described in this patent, it is characterized in that heat treatment magnesium hydroxide is logical
It crosses and magnesium hydrate powder is put into Muffle furnace calcining acquisition, powder meso-position radius is 1~50 μm, preferably 5~30 μm.If in powder
Position diameter is lower than 5 μm, then powder is easy to reunite, it is difficult to disperse；If powder meso-position radius is higher than 30 μm, the easy shape in composite system
At stress concentration point, mechanical properties decrease.
Magnesium hydrate powder is compound with polyester plastics, can assign polyester certain fire-retardant and thermally conductive function, fire retardant mechanism
It is in combustion that magnesium hydroxide, which decomposes, generates magnesia, and releases in conjunction with water, a large amount of latent heat is absorbed, to reduce its institute
Surface temperature of the synthetic material of filling in flame has and polyester is inhibited to decompose and cool down to generated fuel gas
Effect, help to improve the fire resistance of polyester composite, while the vapor released also can be used as a kind of smoke suppressant.Usually
When magnesium hydrate powder additive amount about 50% mass fraction, prepared polyester composite can achieve the fire-retardant of UL-V0
Rank；In terms of another party, it is propagation by thermal phonon in the passage of heat that oxygen, magnesium and hydrogen atom form that magnesium hydroxide is thermally conductive
It realizes, since the atomic weight of hydrogen atom oxygen more therein and magnesium differ greatly, causes the mean free path of its thermal phonon small, thus
Its thermal conductivity is low.
By being heat-treated in advance to magnesium hydrate powder, progress is partially dehydrated, although reducing its flame retardant effect,
The hydrogen content of its passage of heat is reduced, the mean free path of thermal phonon can be increased, to improve its thermal conductivity.The present invention passes through
The temperature and time of control heat treatment magnesium hydroxide, thus controls the dehydration rate of magnesium hydroxide, to realize heat treatment hydroxide
The flame retardant property of magnesium and the adjusting of heating conduction.The present invention with no restrictions, can be conventional Muffle furnace, temperature to high temperature furnace
Control is at 400~700 DEG C, and preferably 500~600 DEG C；1~6h of calcination time, preferably 2~4h.High-temperature calcination is to decompose
Part in magnesium hydroxide combines water, and the decomposition temperature of magnesium hydroxide is 340 DEG C, if temperature is at 400 DEG C hereinafter, dehydration carries out very
Slowly, the dehydration rate time for reaching setting is long；If temperature is higher than 700 DEG C, magnesium hydroxide is dehydrated too fastly, is unfavorable for accurately controlling de-
Water rate, while being unfavorable for keeping the perfection of lattice of powder, increase thermal resistance.
A kind of preparation method of heat conductive flame-retarding polyester composite described in this patent, it is characterized in that polyester base-material is poly- to benzene
Naphthalate (PET) or polybutylene terephthalate (PBT) (PBT), 1~100g/10min of melt index
(2.16kg, 250 DEG C), preferably 20~60g/10min.If melt index is lower than 1g/10min, it is unfavorable for being heat-treated hydroxide
Magnesium powder body is evenly dispersed in base plastic, causes to be difficult to be plasticized extrusion；If melt index is higher than 100g/10min, mechanics
Performance is poor, it is difficult to meet requirement of the application to intensity.
On the basis of being heat-treated magnesium hydroxide conduction powder insulating properties high thermal conductivity powder is added, such as boron nitride, nitrogen in the present invention
Change the compound of aluminium or both, as auxiliary heat conduction agent, to further increase the heating conduction of prepared polyester composite.
The additive amount of auxiliary heat conduction powder does not do special limitation, depending on material prepared is to the desired value of thermal conductivity.In view of nitrogen
Change boron and aluminium nitride more difficult dispersion in the polyester, additive amount, which is maintained within 50phr, to be advisable.
A kind of preparation method of heat conductive flame-retarding polyester composite described in this patent, it is characterized in that auxiliary flame retardant is phosphorous
Compound, preferably Melamine Polyphosphate.In view of heat treatment magnesium hydroxide due to sloughing part in conjunction with water, resistance in advance
Fuel efficiency fruit can be declined, decline degree depending on dehydration rate depending on, therefore, when be heat-treated magnesium hydroxide additive amount it is less high or
When person's dehydration rate is higher, the flame retardant property of prepared polyester composite may not be able to meet application requirement.For this purpose, auxiliary association
The addition for imitating fire retardant it can improve system flame retardant property with synergistic.Phosphonium flame retardant has preferable resistance to oxygen-enriched organic compound
Fuel efficiency fruit, wherein Melamine Polyphosphate is one kind that application range is wider in nitrogen phosphorus flame retardant, and temperature tolerance is good, is decomposed
300 DEG C of temperature or more, gas source (melamine) and acid source (phosphoric acid) substance is generated after decomposition, and there is preferable association with magnesium hydroxide
Effect effect.In combustion process, Melamine Polyphosphate is by the gas and magnesium hydroxide for thermally decomposing generation by thermogenetic water
Steam can dilute the concentration of fuel gas and oxygen；Acid source can be dehydrated into carbon with catalyst, polyester, improve the heated life of magnesium hydroxide
The consistency for producing magnesia carbon-coating, to improve flame retarding efficiency.The additive amount of auxiliary flame retardant regards prepared composite material to resistance
Depending on the requirement of combustion, generally within 30phr.
A kind of preparation method of heat conductive flame-retarding polyester composite described in this patent, it is characterized in that using a kind of special point
Powder, structure have as follows:
R is the alkane segment that carbon atom number is 12-18；
M=2 or 4；
Integer of the n between 2-30.
Dispersing agent is used for the surface treatment of inorganic filler, and the compatibility of resin and inorganic filler can be improved, make composite material
With good mechanical property, and improve processing performance.Polyester group and matrix resin in this kind of dispersing agent have preferable
Compatibility can play the role of interior lubrication, while avoid the migration of dispersing agent；And R is the alkane chain that carbon atom number is 12-18
Section plays the role of dispersing and outer lubrication powder in system.This dispersing agent is added in system, inorganic filler can be improved and exist
The dispersibility of dispersion in polyester, improves the compatibility of powder and resin, and realizes in process simultaneously, inside and outside lubricity
Balance, so that the processing performance of system can be improved.The dosage of this dispersing agent is 3~8phr, and powder additive amount is higher or powder
Partial size is smaller, and dosage is bigger.
The stabilizer that the present invention uses includes one of antioxidant, anti-hydrolysis agent, heat stabilizer or theirs is compound.
Since, containing fatty segment and ester group, under melt-processed or higher temperature, oxygen easily makes in polyester resin main chain
Thermal oxide occurs in it, and so as to cause product jaundice, burnt hair, moisture will cause hydrolysis of ester group, to make polyester physical mechanical property
Decline even destroys.Therefore, in polyester composite process, antioxidant, anti-hydrolysis agent are usually added into, in heat stabilizer
One kind or theirs is compound, prevent polyester from decomposing or degrading under heat, oxygen, water function.Common antioxidant be divided by
Hinder phenols and phosphorous acid lipid, such as antioxidant 1010,168,1076,1098.Heat stabilizer has Ciba company
IrganoxHP136, Irganox1425, IrganoxB2215 etc..Anti-hydrolysis agent has Carbodiimides, such as bright Sheng
Stabaxol-1, Stabaxol-P, Stabaxol-P100, Stabaxol-P200 etc., available, patent does not do special limit
System, additive amount are 1-3 parts.
The present invention is equipped with the powder dispersing agent of special polyester-type based on being heat-treated magnesium hydroxide, provides one kind
The approach with the polyester composite of fire-retardant and thermally conductive function is prepared, it is opposite to be technically characterized by comprising the steps as follows: (1) heat treatment magnesium hydroxide
In common magnesium hydroxide, there is higher thermal conductivity, therefore prepared polyester composite, show more good heat transfer
Performance；(2) different from the thermally conductive and flame retardant polyester implemented respectively at present, heat treatment magnesium hydroxide is realizing the same of thermally conductive function
When, it is able to achieve flame retarding function, especially under thermally conductive more demanding powder height filling situation, prepared polyester composite
Still maintain good flame retardant property；(3) dispersing agent comprising polyester oligomer and long chain alkane used assigns powder and tree
The dispersing uniformity of the better compatibility of rouge and powder in resin, so that the processing performance of composite polyester material is good
Good, the intensity of prepared composite material is high.
Specific implementation formula:
The present invention is further described in detail With reference to embodiment, and the embodiment provided is only for explaining
The bright present invention, the range being not intended to be limiting of the invention.
Raw material sources employed in embodiment and comparative example are described as follows:
Polyester resin (PBT: trade mark B4040G6) is purchased from German BASF；Magnesium hydroxide comes from three water Jin Gexin of Foshan City
Type Materials Co., Ltd；Polyester-type dispersing agent JZF-1, JZF-2, JZF-3 are purchased from Guangzhou Ya Xin Chemical Co., Ltd.；Antioxidant
1010,168 etc. it is purchased from Dongguan City Bao Sheng plastic cement Co., Ltd；IrganoxHP136 is purchased from Ciba；Stabaxol-1 is purchased from
Co., Ltd in bright Sheng chemistry.
Test method employed in embodiment and comparative example is described as follows:
Thermal conductivity: the thermal conductivity of prepared sample, sample are tested using the resistance to laser of speeding of the Germany method conductometer LFA-447 that shines
Size is 1cm*1cm, with a thickness of 2mm.
Flame retardant property: flame retardant property is tested using vertical combustion analyzer CZF-2 (analysis instrument factory of Jiangsu Jiangning county).
Mechanical property: tensile strength is tested using HD-B640DB-S computer servo twin columns puller system.
Embodiment 1
It is heat-treated the preparation of magnesium hydroxide: 1000g magnesium hydrate powder (10 μm of meso-position radius) is put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 550 DEG C, keeps this temperature 4h, obtains heat
Handle powder 648.3g, dehydration rate 35.2%.
The preparation of flame-retarded heat-conducting polyester composite: pressing formula as below, and various raw materials are added in 5L high speed agitator and are mixed
It closes 3 minutes, mixture obtained is added the plasticizing of 35 double screw extruder of φ and is granulated, the temperature setting in each area of extruder are as follows: T1
=190 DEG C, T2=205 DEG C, T3=210 DEG C, T4=210 DEG C, T5=220 DEG C, T6=225 DEG C, T7=225 DEG C, T8=235
DEG C, T9=235 DEG C, mould=220 DEG C T.Pellet obtained is placed 4 hours in 100 DEG C of blast drier, passes through injection molding machine
Prepare test sample.The data tested are shown in Table one.
Comparative example 1
It is heat-treated magnesium hydroxide in 1 polyester composite formula of embodiment and replaces with magnesium hydroxide, other formulas and technique
It is constant.The data tested are shown in Table one.
Comparative example 2
Dispersing agent JZF-1 replaces calcium stearate in 1 polyester composite of embodiment formula, other formulas and technique are constant.
The data tested are shown in Table one.
Embodiment 2
It is heat-treated the preparation of magnesium hydroxide: 1000g magnesium hydrate powder (10 μm of meso-position radius) is put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 500 DEG C, keeps this temperature 4h, obtains heat
Handle powder 762.5g, dehydration rate 23.8%.
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
Embodiment 3
It is heat-treated the preparation of magnesium hydroxide: 1000g magnesium hydrate powder (10 μm of meso-position radius) is put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 450 DEG C, keeps this temperature 4h, obtains heat
Handle powder 864.0g, dehydration rate 13.6%.
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
Embodiment 4
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
Embodiment 5
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
Embodiment 6
It is heat-treated the preparation of magnesium hydroxide: 1000g magnesium hydrate powder (5 μm of meso-position radius) is put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 500 DEG C, keeps this temperature 5h, obtains heat
Handle powder 648.0g, dehydration rate 28.5%.
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
Embodiment 7
It is heat-treated the preparation of magnesium hydroxide: 1000g magnesium hydrate powder (30 μm of meso-position radius) is put into stainless steel disc, powder
The thickness of body is about 3mm, is put into Muffle furnace, and muffle furnace is controlled at 600 DEG C, keeps this temperature 3.6h, is obtained
It is heat-treated powder 648.4g, dehydration rate 28.6%.
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
Embodiment 8
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
Embodiment 9
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
Embodiment 10
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
Embodiment 11
Polyester composite is prepared by formula as below, and technique is the same as embodiment 1.The data tested are shown in Table one.
It can be seen that the test data discovery of (1) comparing embodiment 1-3, comparative example 1 from the test data of table one, it is made
Standby polyester composite, under identical filling number, magnesium hydroxide dehydration rate is higher, and the flame retardant property of composite material is poorer,
Thermal conductivity is higher；(2) comparison of 2 database of embodiment 1 and comparative example shows using polyester-type dispersing agent than common stearic acid
The polyester composite tensile strength of salt preparation is higher, shows this dispersing agent not only and have the good dispersion to powder, and
With the excellent compatibility with resin；(3) number of comparing embodiment 1 and embodiment 4,5 is it has been found that the situation identical in dehydration rate
Under, the filling number of magnesium hydroxide is higher, then the heating conduction of polyester composite is higher, and anti-flammability is better；(4) compare implementation
The number of example 1 and embodiment 6,7 it has been found that with heat treatment magnesium hydrate powder partial size reduction, prepared polyester composite wood
The tensile strength of material increases, and anti-flammability is unchanged, and heating conduction decreases；(5) data pair of embodiment 8 and embodiment 3
Than showing that the addition of Melamine Polyphosphate is remarkably improved the flame retardant property of polyester composite, show it with good
Good flame retardant synergism；(6) nitridation is added it has been found that equally under filling number in the number of comparing embodiment 9,10 and embodiment 3
Boron or boron nitride and aluminium nitride it is compound, be remarkably improved the heating conduction of prepared polyester composite；Further herein
On the basis of compound Melamine Polyphosphate, flame retardant property is obviously improved.
Table one, polyester composite are fire-retardant with heating conduction data
Claims (5)
1. a kind of heat conductive flame-retarding polyester composite, it is characterised in that be made of the component of following parts by weight:
Polyester resin 100
It is heat-treated magnesium hydroxide 100~300
Auxiliary heat conduction agent 0~50
Auxiliary flame retardant 0~30
Dispersing agent 1~8
Stabilizer 1~3
Wherein, heat treatment magnesium hydroxide calcines 1~6h acquisition by the way that magnesium hydrate powder to be put into 400~700 DEG C of high temperature furnace
, powder meso-position radius is 1~50 μm；
Wherein, the structural formula of dispersing agent is as follows:
R is the alkane segment that carbon atom number is 12-18；
M=2 or 4；
Integer of the n between 2-30；
The heat conductive flame-retarding polyester the preparation method comprises the following steps: will material in above-mentioned formula be added mixing 5 in high-speed mixer~
After 30min, it is sent into melting extrusion in double screw extruder, wherein the temperature in each area of double screw extruder are as follows: T1=190~200
DEG C, T2=195~205 DEG C, T3=200~210 DEG C, T4=205~215 DEG C, T5=210~220 DEG C, T6=215~225
DEG C, T7=220~230 DEG C, T8=225~235 DEG C, T9=230~240 DEG C, mould=220~230 DEG C T, the billot squeezed out
Through sink cooling, pelleter granulation is pulled into get heat conductive flame-retarding polyester composite.
2. a kind of heat conductive flame-retarding polyester composite and preparation method thereof according to claim 1, it is characterized in that polyester base-material
It is polyethylene terephthalate (PET) or polybutylene terephthalate (PBT) (PBT), 1~100g/ of melt index
10min。
3. a kind of heat conductive flame-retarding polyester composite and preparation method thereof according to claim 1, it is characterized in that auxiliary heat conduction
Agent is insulating properties high thermal conductivity powder, selected from the compound of boron nitride, aluminium nitride, or both.
4. a kind of heat conductive flame-retarding polyester composite and preparation method thereof according to claim 1, it is characterized in that assisting flame-resistant
Agent is Melamine Polyphosphate.
5. a kind of heat conductive flame-retarding polyester composite and preparation method thereof according to claim 1, it is characterized in that stabilizer is
One of antioxidant, anti-hydrolysis agent, heat stabilizer or theirs is compound.
Priority Applications (1)
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